CN108431197B - Cleaning agent composition and cleaning method - Google Patents
Cleaning agent composition and cleaning method Download PDFInfo
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- CN108431197B CN108431197B CN201680025225.XA CN201680025225A CN108431197B CN 108431197 B CN108431197 B CN 108431197B CN 201680025225 A CN201680025225 A CN 201680025225A CN 108431197 B CN108431197 B CN 108431197B
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- water
- cleaning
- solubility
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- 238000004140 cleaning Methods 0.000 title claims abstract description 137
- 239000012459 cleaning agent Substances 0.000 title claims abstract description 85
- 238000000034 method Methods 0.000 title claims abstract description 35
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000004508 fractional distillation Methods 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- BNRNAKTVFSZAFA-UHFFFAOYSA-N hydrindane Chemical compound C1CCCC2CCCC21 BNRNAKTVFSZAFA-UHFFFAOYSA-N 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
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- 230000010365 information processing Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 150000004715 keto acids Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- HFPZCAJZSCWRBC-UHFFFAOYSA-N p-cymene Chemical compound CC(C)C1=CC=C(C)C=C1 HFPZCAJZSCWRBC-UHFFFAOYSA-N 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 239000006174 pH buffer Substances 0.000 description 1
- 229930006728 pinane Natural products 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000223 polyglycerol Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
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- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
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- 238000004506 ultrasonic cleaning Methods 0.000 description 1
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
- C11D7/5004—Organic solvents
- C11D7/5009—Organic solvents containing phosphorus, sulfur or silicon, e.g. dimethylsulfoxide
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
- C23G5/02—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents
- C23G5/024—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing hydrocarbons
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/0008—Detergent materials or soaps characterised by their shape or physical properties aqueous liquid non soap compositions
- C11D17/0017—Multi-phase liquid compositions
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/0073—Anticorrosion compositions
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
- C11D7/5004—Organic solvents
- C11D7/5013—Organic solvents containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
- C11D7/5004—Organic solvents
- C11D7/5022—Organic solvents containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
- C11D7/5004—Organic solvents
- C11D7/5027—Hydrocarbons
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
- C11D7/5031—Azeotropic mixtures of non-halogenated solvents
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
- C23G5/02—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents
- C23G5/032—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing oxygen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
- C23G5/02—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents
- C23G5/032—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing oxygen-containing compounds
- C23G5/036—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing oxygen-containing compounds having also nitrogen
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
- C23G5/06—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using emulsions
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
- C11D2111/16—Metals
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Detergent Compositions (AREA)
Abstract
The present invention provides a cleaning agent composition and a cleaning method using the cleaning agent, wherein the cleaning agent has excellent environmental safety by containing a predetermined amount of water, can exert excellent cleaning performance, and can effectively inhibit metal corrosion in a cleaned object. A detergent composition for cleaning an object to be cleaned in a cloudy state, comprising 1 st to 4 th organic solvents and water, wherein the 1 st organic solvent is a compound such as a predetermined hydrophobic aromatic compound, the 2 nd organic solvent is a predetermined hydrophobic monohydric alcohol compound, the 3 rd organic solvent is a predetermined hydrophilic nitrogen-containing compound, the 4 th organic solvent is a predetermined hydrophilic amine compound, the amount of water added is in the range of 50 to 3900 parts by weight relative to 100 parts by weight of the total amount of the organic solvents, and the water concentration in the oil phase (measurement temperature: 25 ℃) is 5% by weight or less when the oil phase and the water phase are phase separated.
Description
Technical Field
The present invention relates to a cleaning agent composition and a cleaning method.
In particular, the present invention relates to a cleaning agent composition and a cleaning method which have excellent environmental safety by containing a predetermined amount of water, can exhibit excellent cleaning performance, and can effectively inhibit metal corrosion in an object to be cleaned.
Background
Conventionally, when a semiconductor element, a capacitor, or the like is soldered to a lead frame or the like, it is known that flux is scattered from a solder paste and adheres to the periphery of an electrode as a residue (hereinafter, the residue of flux is referred to as "flux residue").
The flux residue causes not only corrosion at the soldered joint portion but also bonding failure in the wire bonding step or adhesion failure with the molding resin (mold resin) in the resin sealing step, and therefore needs to be removed with a cleaning agent, and various cleaning agents have been proposed (for example, see patent documents 1 to 2).
That is, patent document 1 discloses a cleaning agent composition containing 70% by weight or more of cyclic saturated hydrocarbon having 9 to 18 carbon atoms.
Further, patent document 2 discloses a detergent composition for cleaning an object to be cleaned in a cloudy state, which contains 50 to 1900 parts by weight of water per 100 parts by weight of a detergent composition stock solution, wherein the detergent composition stock solution contains a 1 st organic solvent and a 2 nd organic solvent as organic solvents, the 1 st organic solvent is at least one compound selected from the group consisting of a hydrophobic glycol ether compound, a hydrophobic hydrocarbon compound, a hydrophobic aromatic compound, a hydrophobic ketone compound and a hydrophobic alcohol compound, the 1 st organic solvent has a boiling point in the range of 140 to 190 ℃ and a solubility in water (measurement temperature: 20 ℃) of 50% by weight or less, the 2 nd organic solvent is a hydrophilic amine compound having a boiling point in the range of 140 to 190 ℃ and a solubility in water (measurement temperature: 20 ℃) of more than 50% by weight, the amount of the 2 nd organic solvent is set to a value in the range of 0.3 to 30 parts by weight relative to 100 parts by weight of the 1 st organic solvent, and the amount of the organic solvent having a boiling point exceeding 190 ℃ is set to a value in the range of 0 parts by weight or 0 to 15 parts by weight (wherein 0 part by weight is not included) relative to 100 parts by weight of the 1 st organic solvent.
Patent document 1: japanese laid-open patent publication No. 3-62896 (patent claims)
Patent document 2: WO2012/005068 gazette (claims)
Disclosure of Invention
However, the cleaning agent composition described in patent document 1 is composed of only an organic solvent or only an organic solvent and a surfactant, and has a problem of insufficient environmental safety because water is not added at all.
Further, it is not thought at all that the cleaning agent composition can be made in a cloudy state (emulsion state) by adding water, and the cleaning property can be effectively improved.
On the other hand, the cleaning agent composition described in patent document 2 is used in a cloudy state by adding a relatively large amount of water, and therefore, excellent environmental safety and cleaning performance can be achieved at the same time.
However, the detergent composition described in patent document 2 requires a hydrophilic amine compound, and therefore, the conductivity and pH of the aqueous phase increase, and the object to be cleaned is likely to suffer from metal corrosion.
In particular, when a lead frame obtained by soldering a semiconductor element on which a bonding pad made of aluminum (hereinafter, sometimes referred to as an "aluminum pad") is formed is used as a cleaning object, a problem is found.
That is, in the lead frame, gold and silver constituting the pad, a copper alloy constituting the lead frame body, nickel plating the lead frame body, and various metals such as tin, lead, and silver contained in the solder are similarly bonded by a circuit in addition to aluminum constituting the aluminum pad formed on the semiconductor element.
Therefore, it is known that if such a lead frame is immersed in a conductive cleaning agent composition, a closed circuit is formed, and a metal having a lower potential is sacrificially corroded (hereinafter, such corrosion is referred to as "galvanic corrosion"). According to the "electrochemical potential meter (electrochemical potential meter)", nickel and aluminum have a potential difference of 0.75V, gold and aluminum have a potential difference of 1.05V, and thus, in information processing equipment and the like, a potential difference of 0.35V or more is considered to be a potential difference causing a risk of potential difference corrosion, and aluminum is often a corrosion target at an anode potential.
It is also known that, in corrosion of metals, pH is related to the above potential in addition to the type of electrolyte (hereinafter, such corrosion is referred to as "pH corrosion").
For such corrosion of metals, various "pH-potential maps" are reported, showing metal regions, corrosion regions, and the like.
From the pH-potential diagram of aluminum, it is considered that metallic aluminum becomes aluminate ions (AlO) in an alkaline aqueous solution having a pH of about 9 or more and in an anodic potential state2-) And carrying out dissolution corrosion.
When the lead frame is cleaned with a cleaning agent composition having a pH of 9 or more, which contains an alkaline component such as an amine compound, the lead frame generally has a reduced film thickness of the aluminum pad of about 1 μm or is extremely dissolved and lost, which affects the bondability of the wire bonding.
On the other hand, when only the hydrophilic amine compound is removed from the detergent composition described in patent document 2, not only the detergency is lowered because of the lowered dispersibility of the emulsion, but also the detergency of the hydrophilic amine compound itself is directly balanced, so that there is a problem that it is significantly difficult to maintain the desired detergency.
As a result of intensive studies, the inventors of the present invention have found that the above problems can be solved by blending a predetermined hydrophobic organic solvent as a 1 st organic solvent and a 2 nd organic solvent, a predetermined hydrophilic organic solvent as a 3 rd organic solvent, and water at a predetermined ratio, and by not containing a hydrophilic amine compound as a 4 th organic solvent or having a content of less than a predetermined range, and by setting a water concentration in an oil phase at the time of phase separation to a predetermined range or less, and have completed the present invention.
That is, an object of the present invention is to provide a cleaning agent composition which is excellent in environmental safety and can exhibit excellent cleaning performance and can effectively suppress metal corrosion of an object to be cleaned, and a cleaning method using the cleaning agent.
The present invention solves the above problems and provides a cleaning agent composition for cleaning an object to be cleaned in a cloudy state,
containing 1 st to 4 th organic solvents and water, and
the 1 st organic solvent is at least one compound selected from the group consisting of hydrophobic aromatic compounds, hydrophobic terpene compounds and hydrophobic cycloalkane compounds, the solubility of which in water (measurement temperature: 20 ℃) is 10% by weight or less,
the 2 nd organic solvent is a hydrophobic monohydric alcohol compound having a solubility in water (measurement temperature: 20 ℃) of 10 wt% or less,
the 3 rd organic solvent is either or both of a hydrophilic nitrogen-containing compound and a hydrophilic sulfur-containing compound having a solubility in water (measurement temperature: 20 ℃) of 50 wt% or more,
the 4 th organic solvent is a hydrophilic amine compound having a solubility in water (measurement temperature: 20 ℃) of 50 wt% or more,
the amount of the 2 nd organic solvent is set to a value within the range of 3 to 100 parts by weight based on 100 parts by weight of the 1 st organic solvent,
the amount of the 3 rd organic solvent is set to a value within the range of 3 to 100 parts by weight based on 100 parts by weight of the 1 st organic solvent,
the amount of the 4 th organic solvent is set to a value of less than 0.1 part by weight based on 100 parts by weight of the 1 st organic solvent,
the amount of water is 50 to 3900 parts by weight based on 100 parts by weight of the total amount of organic solvents,
and when the phase separation is carried out between an oil phase and an aqueous phase, the water concentration in the oil phase (measurement temperature: 25 ℃) is set to a value of 5 wt% or less.
That is, in the cleaning agent composition of the present invention, since the predetermined hydrophobic organic solvent, the predetermined hydrophilic organic solvent and water are blended at the predetermined ratio, the oil phase and the aqueous phase can be stably phase-separated, and the object to be cleaned can be cleaned in a cloudy state.
Therefore, the cleaning property by the organic solvent itself in the cleaning agent composition and the clouded state thereof can exert a synergistic effect to obtain an excellent cleaning property.
In addition, since a relatively large amount of water is blended, excellent environmental safety can be obtained.
Further, since the hydrophilic amine compound is not contained or is contained in a range smaller than a predetermined range, even when an object to be cleaned containing a portion made of aluminum or the like is cleaned, the occurrence of metal corrosion can be effectively suppressed.
On the other hand, when the amount of the hydrophilic amine compound to be blended is limited, the detergency tends to be remarkably lowered, but since the composition is a predetermined blending composition and the water concentration in the oil phase is in a predetermined range or less, the excellent detergency can be effectively maintained.
In the present invention, "solubility in water" means the weight% of a solvent that can be dissolved in 100 weight% of water. Therefore, the weight (g) is the same as the weight of the solvent that can be dissolved in 100g of water.
In addition, the organic solvent belonging to both the 1 st organic solvent and the 2 nd organic solvent is classified as the 1 st organic solvent, and the organic solvent belonging to both the 3 rd organic solvent and the 4 th organic solvent is classified as the 4 th organic solvent.
In addition, when the cleaning agent composition of the present invention is constituted, it is preferable that the electrical conductivity (measurement temperature: 25 ℃) in the aqueous phase is set to a value in the range of 0.1 to 300. mu.S/cm.
With this configuration, the occurrence of galvanic corrosion can be suppressed more effectively.
In addition, when the cleaning agent composition of the present invention is constituted, it is preferable that the pH (measurement temperature: 25 ℃) in the aqueous phase is set to a value in the range of 4.5 to 9.5.
With this configuration, the occurrence of pH corrosion can be suppressed more effectively.
In the case of constituting the cleaning agent composition of the present invention, it is preferable that the boiling point of the 1 st organic solvent is set to a value in the range of 140 to 210 ℃, the boiling point of the 2 nd organic solvent is set to a value in the range of 130 to 220 ℃, and the boiling point of the 3 rd organic solvent is set to a value in the range of 150 to 220 ℃.
With such a configuration, the drying property and the regeneration efficiency of the cleaning agent composition after use can be effectively improved.
In addition, in the case of composing the cleaning agent composition of the present invention, it is preferable to set the carbon number of the hydrophobic aromatic compound, the hydrophobic terpene compound and the hydrophobic cycloalkane compound as the 1 st organic solvent to a value within a range of 8 to 10, the hydrogen number to a value within a range of 8 to 20 and the oxygen number to a value within a range of 0 to 1.
With this configuration, the 1 st organic solvent can be brought into a more stable emulsion state, and the cleaning property can be more effectively improved.
In addition, in the case of constituting the cleaning agent composition of the present invention, it is preferable that the hydrophobic monohydric alcohol compound as the 2 nd organic solvent has a carbon number of 6 to 10, a hydrogen number of 8 to 20, and an oxygen number of 1.
With this configuration, the dispersibility of the 1 st organic solvent in an emulsion state with respect to water can be further improved, and the cleaning property can be further improved.
In addition, in the case of constituting the cleaning agent composition of the present invention, it is preferable that the hydrophilic nitrogen-containing compound as the 3 rd organic solvent has a carbon number of 3 to 6, a hydrogen number of 7 to 12, a nitrogen number of 1 and an oxygen number of 1, and it is preferable that the hydrophilic sulfur-containing compound has a carbon number of 2 to 3, a hydrogen number of 6 to 10, a sulfur number of 1 and an oxygen number of 1.
With this configuration, the ionic components derived from the object to be cleaned and the organic acid and salt plasma compounds derived from the flux residue can be effectively dissolved in the aqueous phase, and the cleaning performance can be further improved.
In the case of constituting the cleaning agent composition of the present invention, it is preferable that the hydrophilic amine compound as the 4 th organic solvent has a carbon number of 3 to 7, a hydrogen number of 8 to 16, a nitrogen number of 1 to 3, and an oxygen number of 1.
With this configuration, when particularly high cleaning performance is required, the cleaning performance can be further improved even if a small amount of the surfactant is added.
In the case of constituting the cleaning agent composition of the present invention, it is preferable that the object to be cleaned has at least one metal selected from magnesium, aluminum, phosphorus, titanium, chromium, iron, nickel, copper, zinc, germanium, palladium, silver, indium, tin, antimony, platinum, gold, lead and bismuth, or an alloy containing the metal, on the exposed surface.
Even when such an object to be cleaned is used, the occurrence of metal corrosion can be effectively suppressed.
In another aspect of the present invention, there is provided a cleaning method for cleaning an object to be cleaned by bringing the above-mentioned cleaning agent composition into a cloudy state.
That is, according to the cleaning method of the present invention, since a predetermined cleaning agent composition is used, it is excellent in environmental safety, while it is possible to exhibit excellent cleaning performance, and it is also possible to effectively suppress metal corrosion of the object to be cleaned.
Drawings
FIG. 1 is a graph showing the relationship between the amount of the 4 th organic solvent blended and the electric conductivity and pH in the aqueous phase.
FIG. 2 is a graph for explaining the relationship between the amount of the 4 th organic solvent to be added and the metal corrosion resistance and the cleaning property.
Fig. 3 is a graph for explaining the relationship between the water concentration in the oil phase and the detergency.
Fig. 4 (a) to (b) are views for explaining an example of the cleaning apparatus.
Fig. 5 (a) to (b) are views for explaining test pieces for evaluating metal corrosion resistance.
Detailed Description
[ embodiment 1]
containing 1 st to 4 th organic solvents and water, and
the 1 st organic solvent is at least one compound selected from the group consisting of hydrophobic aromatic compounds, hydrophobic terpene compounds and hydrophobic cycloalkane compounds, the solubility of which in water (measurement temperature: 20 ℃) is 10% by weight or less,
the 2 nd organic solvent is a hydrophobic monohydric alcohol compound having a solubility in water (measurement temperature: 20 ℃) of 10 wt% or less,
the 3 rd organic solvent is either or both of a hydrophilic nitrogen-containing compound and a hydrophilic sulfur-containing compound having a solubility in water (measurement temperature: 20 ℃) of 50 wt% or more,
the 4 th organic solvent is a hydrophilic amine compound having a solubility in water (measurement temperature: 20 ℃) of 50 wt% or more,
the amount of the 2 nd organic solvent is set to a value within the range of 3 to 100 parts by weight based on 100 parts by weight of the 1 st organic solvent,
the amount of the 3 rd organic solvent is set to a value within the range of 3 to 100 parts by weight based on 100 parts by weight of the 1 st organic solvent,
the 4 th organic solvent is added in an amount of less than 0.1 part by weight based on 100 parts by weight of the 1 st organic solvent,
the amount of water is 50 to 3900 parts by weight based on 100 parts by weight of the total amount of organic solvents,
and when the phase separation is carried out between an oil phase and an aqueous phase, the water concentration in the oil phase (measurement temperature: 25 ℃) is set to a value of 5 wt% or less.
1. 1 st organic solvent
The 1 st organic solvent constituting the detergent composition of the present invention is at least one compound selected from the group consisting of hydrophobic aromatic compounds, hydrophobic terpene compounds and hydrophobic cycloalkane compounds, and has a solubility in water (measurement temperature: 20 ℃) of 10 wt% or less.
The 1 st organic solvent contributes to the effect of the 2 nd and 3 rd organic solvents described later and is in an emulsion state, and the cleaning agent composition is in a cloudy state.
In addition, the 1 st organic solvent is excellent in dissolving ability for flux residue, and therefore, the cleaning property can be effectively improved.
Therefore, the 1 st organic solvent originally has excellent cleaning properties and has a synergistic effect of being in an emulsion state, and thus has an effect of imparting excellent cleaning properties to the cleaning agent composition.
(1) Species of
Characterized in that the 1 st organic solvent is at least one compound selected from the group consisting of a hydrophobic aromatic compound, a hydrophobic terpene compound and a hydrophobic cycloalkane compound.
More specifically, examples thereof include indene (boiling point: 182 ℃ C., solubility in water: 1 wt% or less), hemimellitene (boiling point: 176 ℃ C., solubility in water: 1 wt% or less), hemimellitene (boiling point: 169 ℃ C., solubility in water: 1 wt% or less), mesitylene (boiling point: 165 ℃ C., solubility in water: 1 wt% or less), cumene (boiling point: 152 ℃ C., solubility in water: 1 wt% or less), methylisopropylene (boiling point: 177 ℃ C., solubility in water: 1 wt% or less), phenetole (boiling point: 173 ℃ C., solubility in water: 1 wt% or less), limonene (solubility in water: 176 ℃ C., 1 wt% or less), alpha-pinene (for example, a turpentine oil containing a main component) (boiling point: 155 to 156 ℃ C., solubility in water: 1 wt% or less), To pair
An alkane (boiling point: 168 ℃ C., solubility in water: 1% by weight or less), decahydronaphthalene (boiling point: 186 ℃ C., solubility in water: 1% by weight or less), octahydroindene (boiling point: 159 ℃ C., solubility in water: 1% by weight or less), pinane (boiling point: 167 ℃ C., solubility in water: 1% by weight or less), and paraffine
Mixtures of diene isomers (e.g., japanese terpenoid chemical plant formula)Manufactured by japan, Dipentene T) (boiling point: 168-182 ℃, solubility in water: 1% by weight or less), a mixture of C9 alkylcyclohexane (e.g., Spclean 150, manufactured by pillarville petrochemical co., ltd.) (boiling point: solubility in water at 145-170 ℃: 1% by weight or less), and the like.
In addition, the number of carbon atoms in the hydrophobic aromatic compound, the hydrophobic terpene compound and the hydrophobic cycloalkane compound as the 1 st organic solvent is preferably in the range of 8 to 10, the number of hydrogen atoms is preferably in the range of 8 to 20, and the number of oxygen atoms is preferably in the range of 0 to 1.
This is because the 1 st organic solvent can be more stably brought into an emulsion state and the cleaning property can be more effectively improved by such a compound.
Therefore, among the above-mentioned 1 st organic solvents, those selected from the group consisting of indene, methylisopropylene, cumene, phenetole, decahydronaphthalene and p-naphthalene are particularly preferable
At least one compound of an alkane.
(2) Solubility in water
The method is characterized in that the solubility of the 1 st organic solvent in water (measurement temperature: 20 ℃) is 10 wt% or less.
The reason for this is that if the solubility is a value exceeding 10% by weight, it is difficult to adjust the water concentration in the oil phase to a predetermined range or less, and it may be difficult to sufficiently exhibit the excellent cleaning property which the 1 st organic solvent originally has in a state where the organic solvent does not contain water.
Therefore, the upper limit of the solubility of the 1 st organic solvent in water (measurement temperature: 20 ℃) is more preferably 5% by weight or less, and still more preferably 3% by weight or less.
(3) Boiling point
In addition, the boiling point of the 1 st organic solvent is preferably within a range of 140 to 210 ℃.
The reason for this is that if the boiling point is less than 140 ℃, the amount of volatilization at the time of use increases, the amount of liquid consumption increases, and the economy deteriorates.
On the other hand, if the boiling point is a value exceeding 210 ℃, the drying property is deteriorated, and poor drying is likely to occur and remain in the object to be cleaned. In addition, if the drying property is to be improved, an excessive amount of heat energy must be applied to the object to be cleaned during drying. Further, when the used detergent composition is regenerated by fractional distillation, the energy required for regeneration may become excessively large, or the high boiling point component may not be distilled off during regeneration, and the recovery rate of the detergent composition may be lowered, or the regeneration efficiency may be easily lowered, for example, a detergent composition having a predetermined composition may not be obtained. Further, since the heating temperature at the time of fractionating the used detergent composition becomes high, the components of the detergent composition are likely to be decomposed, and the cleaning property of the regenerated detergent composition is lowered, and it is difficult to stably obtain a detergent composition having a sufficient cleaning property.
Therefore, the lower limit of the boiling point of the 1 st organic solvent is more preferably set to a value of 145 ℃ or higher, and still more preferably set to a value of 150 ℃ or higher.
The upper limit of the boiling point of the 1 st organic solvent is more preferably 200 ℃ or lower, and still more preferably 190 ℃ or lower.
(4) Compounding amount
The amount of the 1 st organic solvent to be mixed is preferably in the range of 40 to 90% by weight based on the total amount (100% by weight) of the organic solvent portion of the detergent composition (hereinafter, may be referred to as "stock solution for a detergent composition").
The reason for this is that if the amount is less than 40% by weight, phase separation is difficult to occur, making it difficult to obtain a cloudy state, and the cleaning performance may be excessively reduced.
On the other hand, if the amount of the surfactant is more than 90% by weight, the oil phase and the water phase may be separated too strongly, and it may be difficult to obtain a stably cloudy state, and the cleaning property may be easily deteriorated.
Therefore, the lower limit of the amount of the 1 st organic solvent is preferably 45% by weight or more, more preferably 50% by weight or more, based on the total amount (100% by weight) of the raw liquid for a cleaning agent composition.
The upper limit of the amount of the 1 st organic solvent is preferably 80% by weight or less, more preferably 75% by weight or less, based on the total amount (100% by weight) of the raw liquid for a cleanser composition.
2. 2 nd organic solvent
The 2 nd organic solvent of the present invention is a hydrophobic monohydric alcohol compound having a solubility in water (measurement temperature: 20 ℃) of 10% by weight or less.
The 2 nd organic solvent is blended with the 1 st organic solvent in an emulsion state and water from the oil phase side, and contributes to improvement of the dispersion state of the emulsion, and the 2 nd organic solvent is particularly excellent in solubility in rosin.
Therefore, the 2 nd organic solvent has a function of assisting the 1 st organic solvent in an emulsion state from the oil phase side, and improving the cleaning property of the cleaning agent composition.
(1) Species of
Characterized in that the 2 nd organic solvent is a hydrophobic monohydric alcohol compound.
More specifically, examples thereof include 1-hexanol (boiling point: 157 ℃ C., solubility in water: 1% by weight or less), methylpentanol (boiling point: 131 ℃ C., solubility in water: 1.6% by weight), 2-ethylbutanol (boiling point: 147 ℃ C., solubility in water: 1% by weight), methylisobutylcarbinol (boiling point: 131 ℃ C., solubility in water: 1.5% by weight), cyclohexanol (boiling point: 161 ℃ C., solubility in water: 3.6% by weight), 1-heptanol (boiling point: 175 ℃ C., solubility in water: 1% by weight or less), 2-heptanol (boiling point: 160 ℃ C., solubility in water: 1% by weight or less), 3-heptanol (boiling point: 156 ℃ C., solubility in water: 1% by weight or less), 4-heptanol (boiling point: 156 ℃ C., solubility in water: 1% by weight or less), and mixtures thereof, 2-methylcyclohexanol (boiling point: 173 ℃ C., solubility in water: 1% by weight or less), benzyl alcohol (boiling point: 206 ℃ C., solubility in water: 4.3% by weight), 1-octanol (boiling point: 195 ℃ C., solubility in water: 1% by weight or less), 2-octanol (boiling point: 178 ℃ C., solubility in water: 1% by weight or less), 2-ethylhexanol (boiling point: 184 ℃ C., solubility in water: 1% by weight or less), 2-nonanol (boiling point: 193 ℃ C., solubility in water: 1% by weight or less), diisobutylcarbinol (boiling point: 176 ℃ C., solubility in water: 1% by weight or less), 3,5, 5-trimethylhexanol (boiling point: 194 ℃ C., solubility in water: 1% by weight or less), terpineol (boiling point: 217 ℃ C., solubility in water: 1% by weight or less), and the like.
In addition, the number of carbon atoms in the hydrophobic monohydric alcohol compound as the 2 nd organic solvent is preferably in the range of 6 to 10, the number of hydrogen atoms is preferably in the range of 8 to 20, and the number of oxygen atoms is preferably 1.
The reason for this is that if such a compound is used, the dispersibility of the 1 st organic solvent in the emulsion state in water can be further improved, and the cleaning property can be further improved.
Therefore, among the above-mentioned 2 nd organic solvent, at least one compound selected from the group consisting of 1-hexanol, cyclohexanol, 1-heptanol, 2-heptanol, benzyl alcohol, 1-octanol, diisobutyl methanol and terpineol is particularly preferable.
(2) Solubility in water
The method is characterized in that the solubility of the 2 nd organic solvent in water (measurement temperature: 20 ℃) is 10 wt% or less.
The reason for this is that if the solubility is a value exceeding 10% by weight, it may be difficult to blend the 1 st organic solvent in an emulsion state with water from the oil phase side to improve the dispersibility of the emulsion and thus improve the cleaning property.
Further, it may be difficult to adjust the water concentration in the oil phase to a predetermined range or less, and it may be difficult to sufficiently exhibit the excellent cleaning property which is originally possessed in a state where the 1 st organic solvent and the 2 nd organic solvent do not contain water.
Therefore, the upper limit of the solubility of the 2 nd organic solvent in water (measurement temperature: 20 ℃) is more preferably 7% by weight or less, and still more preferably 5% by weight or less.
(3) Boiling point
In addition, the boiling point of the 2 nd organic solvent is preferably in the range of 130 to 220 ℃.
The reason for specifying the boiling point of the 2 nd organic solvent is the same as the reason for specifying the boiling point of the 1 st organic solvent.
Therefore, the lower limit of the boiling point of the 2 nd organic solvent is set to a value of more preferably 140 ℃ or higher, and still more preferably 150 ℃ or higher.
The upper limit of the boiling point of the 2 nd organic solvent is more preferably 215 ℃ or lower, and still more preferably 210 ℃ or lower.
(4) Compounding amount
The method is characterized in that the amount of the 2 nd organic solvent is within a range of 3 to 100 parts by weight based on 100 parts by weight of the 1 st organic solvent.
The reason for this is that if the amount of the above-mentioned compound is less than 3 parts by weight, the absolute amount of the 2 nd organic solvent to the 1 st organic solvent is insufficient, and it may be difficult to blend the 1 st organic solvent in an emulsion state with water from the oil phase side to improve the dispersibility of the emulsion and thus the cleaning property.
In addition, it may be difficult to obtain excellent cleaning properties inherent in the 2 nd organic solvent.
On the other hand, if the amount exceeds 100 parts by weight, phase separation is less likely to occur, making it difficult to obtain a cloudy state, and the cleaning performance tends to be excessively lowered.
Therefore, the lower limit of the amount of the 2 nd organic solvent is preferably 7 parts by weight or more, and more preferably 10 parts by weight or more, based on 100 parts by weight of the 1 st organic solvent.
The upper limit of the amount of the 2 nd organic solvent is preferably 90 parts by weight or less, and more preferably 80 parts by weight or less, based on 100 parts by weight of the 1 st organic solvent.
3.3 rd organic solvent
The 3 rd organic solvent of the present invention is a hydrophilic nitrogen-containing compound and a hydrophilic sulfur compound having a solubility in water (measurement temperature: 20 ℃) of 50 wt% or more, or either one of them.
The 3 rd organic solvent can sufficiently dissolve the ionic components derived from the object to be cleaned and the organic acid and salt plasma compounds derived from the flux residue in the aqueous phase, and contributes to improving the dispersibility of the emulsion by adjusting the 1 st organic solvent, the 2 nd organic solvent and water from the aqueous phase side.
Therefore, the 3 rd organic solvent has a function of improving the cleaning property of the cleaning agent composition by assisting the 1 st organic solvent in an emulsion state from the aqueous phase side.
(1) Species of
Characterized in that the 3 rd organic solvent is a hydrophilic nitrogen-containing compound and a hydrophilic sulfur-containing compound or any one of the compounds.
In addition, the 3 rd organic solvent, which is a hydrophilic nitrogen-containing compound, is preferably such that the number of carbon atoms is in the range of 3 to 6, the number of hydrogen atoms is in the range of 7 to 12, the number of nitrogen atoms is 1, and the number of oxygen atoms is 1, and the hydrophilic sulfur-containing compound is preferably such that the number of carbon atoms is in the range of 2 to 3, the number of hydrogen atoms is in the range of 6 to 10, the number of sulfur atoms is 1, and the number of oxygen atoms is 1.
This is because if such a compound is used, the cleaning performance can be further improved by effectively dissolving the organic acid/salt type plasma compound derived from the flux residue and the ionic component derived from the object to be cleaned in the aqueous phase.
More specifically, N-methyl-2-pyrrolidone (boiling point: 204 ℃ C., solubility in water: 100% by weight or more), N-ethyl-2-pyrrolidone (boiling point: 218 ℃ C., solubility in water: 100% by weight or more), dimethyl sulfoxide (boiling point: 189 ℃ C., solubility in water: 100% by weight or more), dimethylacetamide (boiling point: 166 ℃ C., solubility in water: 100% by weight or more), N-dimethylformamide (boiling point: 153 ℃ C., solubility in water: 100% by weight or more), N-diethylformamide (boiling point: 177 ℃ C., solubility in water: 100% by weight or more) and the like are preferable.
(2) Solubility in water
The solubility of the 3 rd organic solvent in water (measurement temperature: 20 ℃) is 50 wt% or more.
The reason for this is that if the solubility is less than 50% by weight, it may be difficult to sufficiently dissolve the ionic component derived from the object to be cleaned in the aqueous phase.
In addition, it is sometimes difficult to blend the 1 st organic solvent and the 2 nd organic solvent in an emulsion state with water from the aqueous phase side to improve the dispersibility of the emulsion and to improve the cleaning property.
Therefore, the lower limit of the solubility of the 3 rd organic solvent in water (measurement temperature: 20 ℃) is more preferably 60% by weight or more, and still more preferably 70% by weight or more.
The upper limit of the solubility of the 3 rd organic solvent in water (measurement temperature: 20 ℃) is not particularly limited, but is preferably infinite (∞).
(3) Boiling point
In addition, preferably, the 3 rd organic solvent has a boiling point in the range of 150 to 220 ℃.
The reason for specifying the boiling point of the 3 rd organic solvent is the same as the reason for specifying the boiling point of the 1 st organic solvent.
Therefore, the lower limit of the boiling point of the 3 rd organic solvent is more preferably 155 ℃ or higher, and still more preferably 160 ℃ or higher.
The upper limit of the boiling point of the 3 rd organic solvent is more preferably 215 ℃ or lower, and still more preferably 210 ℃ or lower.
(4) Compounding amount
The amount of the 3 rd organic solvent is set to a value within a range of 3 to 100 parts by weight based on 100 parts by weight of the 1 st organic solvent.
The reason for this is that if the amount is less than 3 parts by weight, the absolute amount of the 3 rd organic solvent to the 1 st organic solvent is insufficient, and it may be difficult to sufficiently dissolve the organic acid/salt type plasma compound derived from the flux residue and the ionic component derived from the object to be cleaned in the aqueous phase.
In addition, it is sometimes difficult to blend the 1 st organic solvent and the 2 nd organic solvent in an emulsion state with water from the aqueous phase side to improve the dispersibility of the emulsion and to improve the cleaning property.
Further, the reason is that the surface tension of the aqueous phase is excessively increased, and the cleaning property of the gaps of the object to be cleaned is lowered, or it is difficult to obtain good liquid removal property and drying property.
On the other hand, if the amount exceeds 100 parts by weight, phase separation is less likely to occur, making it difficult to obtain a cloudy state, and the cleaning performance tends to be excessively lowered.
Therefore, the lower limit of the amount of the 3 rd organic solvent is preferably 5 parts by weight or more, and more preferably 7 parts by weight or more, based on 100 parts by weight of the 1 st organic solvent.
The upper limit of the amount of the 3 rd organic solvent is preferably 90 parts by weight or less, and more preferably 80 parts by weight or less, based on 100 parts by weight of the 1 st organic solvent.
4. 4 th organic solvent
The 4 th organic solvent of the present invention is a hydrophilic amine compound having a solubility in water (measurement temperature: 20 ℃) of 50 wt% or more.
The 4 th organic solvent is added to the metal to improve the metal corrosion resistance, but is added to the metal to obtain higher cleaning performance.
That is, when the 4 th organic solvent is added, the electric conductivity and pH of the aqueous phase become high, and therefore, the object to be cleaned is likely to be corroded by a potential difference or by pH.
On the other hand, the 4 th organic solvent contributes to improving the dispersibility of the emulsion by blending the 1 st organic solvent in an emulsion state and water from the water phase side, and can effectively dissolve the ionic components derived from the object to be cleaned and the organic acid and salt type plasma compounds derived from flux residue in the water phase.
Therefore, the 4 th organic solvent can be blended in a range in which metal corrosion can be suppressed to such an extent that it is practically not problematic, and particularly excellent cleaning properties can be obtained.
(1) Species of
Characterized in that the 4 th organic solvent is a hydrophilic amine compound.
More specifically, N-ethylpiperazine (boiling point: 157 ℃ C., solubility in water: 100% by weight or more), N-diethylisopropanolamine (boiling point: 159 ℃ C., solubility in water: 100% by weight or more), N-methylethanolamine (boiling point: 160 ℃ C., solubility in water: 100% by weight or more), monoisopropanolamine (boiling point: 160 ℃ C., solubility in water: 100% by weight or more), N-diethylethanolamine (boiling point: 162 ℃ C., solubility in water: 100% by weight or more), N-ethylethanolamine (boiling point: 169 ℃ C., solubility in water: 100% by weight or more), N-t-butylethanolamine (boiling point: 175 ℃ C., solubility in water: 100% by weight or more), 1-amino-4-methylpiperazine (boiling point: 178 ℃, solubility in water: 100% by weight or more), N-aminoethylpiperazine (boiling point: solubility in water at 182 ℃: 100% by weight or more), benzylamine (boiling point: 185 ℃, solubility in water: 100% by weight or more), N-allylpiperazine (boiling point: 185 ℃, solubility in water: 100% by weight or more), and the like.
In addition, the 4 th organic solvent, which is a hydrophilic amine compound, is preferably such that the number of carbon atoms is in the range of 3 to 7, the number of hydrogen atoms is in the range of 8 to 16, the number of nitrogen atoms is in the range of 1 to 3, and the number of oxygen atoms is 1.
The reason for this is that if such a 4 th organic solvent is used, the cleaning property can be further improved even if a small amount of the solvent is added when an object to be cleaned, which requires particularly high cleaning property, is cleaned.
Therefore, among the above-mentioned 4 th organic solvent, it is particularly preferable to use at least one compound selected from the group consisting of N, N-diethylisopropanolamine, N-ethylethanolamine, N-methylethanolamine, benzylamine and monoisopropanolamine.
(2) Solubility in water
The method is characterized in that the solubility of the 4 th organic solvent in water (measurement temperature: 20 ℃) is 50% by weight or more.
The reason for this is that if the solubility is less than 50 wt%, the 4 th organic solvent is mixed in the hard phase, but the organic acid/salt type plasma compound derived from flux residue and the ionic component derived from the object to be cleaned are not easily dissolved in the aqueous phase in some cases, because the organic solvent is taken up by the oil phase side, from the viewpoint of further improving the cleaning performance.
In addition, it is sometimes difficult to improve the dispersibility of the emulsion and thus the cleaning property by mixing the 1 st organic solvent or the like in an emulsion state with water from the aqueous phase side.
Therefore, the lower limit of the solubility of the 4 th organic solvent in water (measurement temperature: 20 ℃) is more preferably 60% by weight or more, and still more preferably 70% by weight or more.
The upper limit of the solubility of the 4 th organic solvent in water (measurement temperature: 20 ℃) is not particularly limited, but is preferably infinite (∞).
(3) Boiling point
Further, the boiling point of the 4 th organic solvent is preferably set to a value within the range of 140 to 200 ℃.
The reason for fixing the boiling point of the 4 th organic solvent is the same as the reason for specifying the boiling point of the 1 st organic solvent.
Therefore, the lower limit of the boiling point of the 4 th organic solvent is more preferably set to a value of 145 ℃ or higher, and still more preferably set to a value of 150 ℃ or higher.
The upper limit of the boiling point of the 4 th organic solvent is preferably 195 ℃ or lower, more preferably 185 ℃ or lower.
(4) Compounding amount
The method is characterized in that the amount of the 4 th organic solvent is less than 0.1 part by weight per 100 parts by weight of the 1 st organic solvent.
The reason for this is that if the amount of the above-mentioned component is 0.1 part by weight or more, the conductivity and pH of the aqueous phase may be increased, and the metal corrosion of the object to be cleaned may easily occur.
In particular, when a lead frame obtained by die bonding a semiconductor element having an aluminum pad is used as a subject to be cleaned, since potential difference corrosion and pH corrosion occur simultaneously, the aluminum pad having a thickness of about 1 μm is usually dissolved, and it is sometimes difficult to stably obtain electrical conduction in a final product.
Therefore, the upper limit of the amount of the 4 th organic solvent is preferably 0.07 parts by weight or less, more preferably 0.05 parts by weight or less, and most preferably 0 parts by weight, i.e., no amount is added, based on 100 parts by weight of the 1 st organic solvent.
Among them, when cleaning an object to be cleaned which requires particularly high cleaning performance, such as an in-vehicle component or a high-frequency component which requires high reliability, a semiconductor package substrate which is mounted at high density, or the like, it is preferable to mix a very small amount of the 4 th organic solvent in a range in which metal corrosion can be suppressed to a level which is practically not problematic.
In this case, the lower limit of the amount of the 4 th organic solvent is preferably 0.01 parts by weight or more, more preferably 0.03 parts by weight or more, and still more preferably 0.05 parts by weight or more, based on 100 parts by weight of the 1 st organic solvent.
Next, the relationship between the amount of the 4 th organic solvent to be added and the electric conductivity and pH of the aqueous phase will be described with reference to fig. 1.
That is, FIG. 1 shows a characteristic curve A in which the horizontal axis represents the amount of the 4 th organic solvent (part by weight) relative to 100 parts by weight of propylene glycol monobutyl ether in the cleanser composition based on comparative example 6, the electrical conductivity (. mu.S/cm) at 25 ℃ in the aqueous phase on the left vertical axis, and a characteristic curve B in which the pH (-) at 25 ℃ in the aqueous phase on the right vertical axis.
The details of the methods for measuring the conductivity and pH in the aqueous phase are described in the examples.
Comparative example 6 corresponds to a conventional cloudy detergent composition containing a hydrophilic amine compound as an essential component.
From the above-mentioned characteristic curves A and B of FIG. 1, it is understood that the conductivity and pH of the aqueous phase monotonously increase as the amount of the 4 th organic solvent to be added increases.
More specifically, as shown in the characteristic curve A, it is found that if the 4 th organic solvent is added in an amount of 0.1 part by weight or more, the electric conductivity in the aqueous phase becomes 120. mu.S/cm or more.
Further, as shown in the characteristic curve B, it is found that if the amount of the 4 th organic solvent is 0.1 parts by weight or more, the pH in the aqueous phase is increased to a value of 9.6 or more.
Therefore, as described with reference to fig. 2, the 4 th organic solvent is added in an increased amount, which tends to cause potential difference corrosion due to high conductivity and pH corrosion due to high pH.
Next, the relationship between the amount of the 4 th organic solvent to be added and the metal corrosion resistance and the cleaning property will be described with reference to fig. 2.
That is, fig. 2 shows a characteristic curve a in which the horizontal axis represents the amount of the 4 th organic solvent (part by weight) relative to 100 parts by weight of propylene glycol monobutyl ether in the cleaner composition based on comparative example 6, the left vertical axis represents the metal corrosion resistance (relative value), and the right vertical axis represents the cleaning property (relative property).
Here, the evaluation results (relative values) of corrosion resistance are represented by evaluation scores of 0 to 10, and the evaluation criteria are as follows.
Evaluation score 10: no change in appearance was observed after 60 minutes of immersion.
Evaluation score 9: no change in appearance was seen after 45 minutes of immersion, but a change in appearance was seen after 60 minutes of immersion.
Evaluation score 8: no change in appearance was seen after 30 minutes of immersion, but a change in appearance was seen after 45 minutes of immersion.
Evaluation score 7: no change in appearance was seen after 25 minutes of immersion, but a change in appearance was seen after 30 minutes of immersion.
Evaluation score 6: no change in appearance was seen after 20 minutes of immersion, but a change in appearance was seen after 25 minutes of immersion.
Evaluation score 5: no change in appearance was seen after 15 minutes of immersion, but a change in appearance was seen after 20 minutes of immersion.
Evaluation score 4: no change in appearance was seen after 10 minutes of immersion, but a change in appearance was seen after 15 minutes of immersion.
Evaluation score 3: no change in appearance was seen after 5 minutes of immersion, but a change in appearance was seen after 10 minutes of immersion.
Evaluation score 2: no change in appearance was seen after 3 minutes of immersion, but a change in appearance was seen after 5 minutes of immersion.
Evaluation score 1: no change in appearance was observed after 1 minute of immersion, but a change in appearance was observed after 3 minutes of immersion.
Evaluation score 0: after 1 minute of immersion, a change in appearance was seen.
The evaluation results (relative values) of the cleanability were represented by evaluation scores of 0 to 10, and the evaluation criteria were as follows.
Evaluation score 10: the cleaning time of the soldering flux is 0 to less than 10 minutes.
Evaluation score 9: the cleaning time of the soldering flux is 10 to less than 12 minutes.
Evaluation score 8: the cleaning time of the soldering flux is 12 to less than 15 minutes.
Evaluation score 7: the cleaning time of the soldering flux is 15-less than 17 minutes.
Evaluation score 6: the cleaning time of the soldering flux is 17-20 minutes.
Evaluation score 5: the cleaning time of the soldering flux is 20 to less than 25 minutes.
Evaluation score 4: the cleaning time of the soldering flux is 25 to less than 30 minutes.
Evaluation score 3: the cleaning time of the soldering flux is 30-less than 40 minutes.
Evaluation score 2: the cleaning time of the soldering flux is 40 to less than 50 minutes.
Evaluation score 1: the cleaning time of the soldering flux is 50 to less than 60 minutes.
Evaluation score 0: the cleaning time of the soldering flux is more than 60 minutes.
The details of the evaluation method of the metal corrosion resistance and the cleaning property are described in examples.
From the above-mentioned characteristic curves a and B of fig. 2, it is understood that the evaluation score of the metal corrosion resistance is decreased as the content of the 4 th organic solvent is increased, while the evaluation score of the cleaning property is increased as the content of the 4 th organic solvent is increased.
More specifically, as shown in the characteristic curve a, it is found that the evaluation value of the metal corrosion resistance is 10 when the amount of the 4 th organic solvent is 0 parts by weight, but if the amount of the 4 th organic solvent is 1 part by weight or more, the evaluation value of the metal corrosion resistance is rapidly decreased to 1.
On the other hand, as shown in the characteristic curve B, it is found that the evaluation value of the cleaning property is 0 when the amount of the 4 th organic solvent is 0 parts by weight, but if the amount of the 4 th organic solvent is 0.4 parts by weight or more, the evaluation value of the cleaning property rapidly increases to 10.
Therefore, it is found that it is very difficult to obtain both metal corrosion resistance and cleaning performance in the case of a conventional cloudy cleaning agent composition containing a hydrophilic amine compound as an essential component.
On the other hand, FIG. 2 shows a graph C showing the metal corrosion resistance and a graph D showing the cleaning property of the cleaning agent composition of example 1, in addition to the characteristic curves A and B.
From the above-mentioned graphs C and D, it is understood that the cleaning agent composition of the present invention can exhibit excellent cleaning properties even when the hydrophilic amine compound is not contained at all, and thus can achieve both excellent metal corrosion resistance and excellent cleaning properties.
5. Other Compounds
The cleaning agent composition of the present invention may contain compounds other than the 1 st to 4 th organic solvents as long as the effects of the present invention are not impaired.
Such a compound is not particularly limited, and examples thereof include a hydrophobic glycol ether compound, a hydrophobic amine compound, and a surfactant.
Examples of the hydrophobic glycol ether compound include propylene glycol monobutyl ether and dipropylene glycol dimethyl ether.
Examples of the hydrophobic amine compound include dibutylamine, 2-ethylhexylamine, triallylamine, and dimethylbenzylamine.
Examples of the surfactant include polyoxyethylene alkyl ethers, polyoxyethylene alkylphenyl ethers, polyoxyethylene polypropylene alkyl ethers, polyoxyethylene sorbitan fatty acid esters, polyoxyethylene glycol fatty acid esters, polyoxyethylene alkylamines, polyoxyethylene benzyl alcohols, and polyglycerol fatty acid esters.
In addition, particularly when the 4 th organic solvent is blended, it is preferable to blend a pH buffer, a pH adjuster, a rust inhibitor, an antioxidant, and the like from the viewpoint of more effectively suppressing the occurrence of metal corrosion.
The amount of the other compound is preferably in the range of 0.1 to 10 parts by weight, and more preferably in the range of 1 to 7 parts by weight, based on 100 parts by weight of the 1 st organic solvent.
6. Water (W)
The cleaning agent composition of the present invention is characterized by containing water in an amount within a range of 50 to 3900 parts by weight relative to 100 parts by weight of the total amount of the organic solvents.
The reason for this is that if the amount of water is less than 50 parts by weight, not only the cleaning property may be reduced, but also the cleaning agent composition may be made uniform, and it may be difficult to make the cleaning agent composition in a cloudy state.
On the other hand, if the amount of water is more than 3900 parts by weight, the organic solvent is excessively diluted, and the cleaning property may be remarkably lowered.
Therefore, the lower limit of the amount of water is more preferably 75 parts by weight or more, and still more preferably 100 parts by weight or more.
The upper limit of the amount of water to be added is more preferably 1900 parts by weight or less, and still more preferably 900 parts by weight or less.
7. Characteristics of liquid
(1) Water concentration in oil phase
The cleaning agent composition of the present invention is characterized in that when the composition is separated into an oil phase and an aqueous phase, the water concentration in the oil phase (measurement temperature: 25 ℃) is set to a value of 5% by weight or less.
The reason for this is that, although the detergency tends to be remarkably lowered when the amount of the hydrophilic amine compound to be added is limited from the viewpoint of suppressing metal corrosion, the excellent detergency can be effectively maintained by assuming the above-mentioned predetermined blending composition and setting the water concentration in the oil phase to a predetermined range or less.
That is, if the water concentration is a value exceeding 5% by weight, it becomes difficult for the 1 st organic solvent or the 2 nd organic solvent constituting the oil phase to sufficiently exhibit the excellent cleaning property which is originally possessed in a state of not containing water.
More specifically, if the 1 st organic solvent or the 2 nd organic solvent constituting the oil phase contains a predetermined amount of water or more, the dissolving ability of the nonpolar compound such as rosin derived from the flux residue is lowered, and the cleaning property is remarkably lowered.
Therefore, the water concentration in the oil phase (measurement temperature: 25 ℃) is set to a value of more preferably 3% by weight or less, and still more preferably 1.5% by weight or less.
In the present invention, "water concentration in the oil phase" means the saturated water concentration of the oil phase.
Next, the relationship between the water concentration in the oil phase and the washability will be described with reference to fig. 3.
That is, fig. 3 shows a characteristic curve in which the horizontal axis represents the water concentration (weight%) of the oil phase in the cleanser composition according to example 3 at 25 ℃ and the vertical axis represents the cleansing performance (relative value).
The criteria for the evaluation results of the cleanability and the like are the same as in the case of fig. 2.
From the characteristic curve of fig. 3, it is understood that the detergency decreases as the water concentration in the oil phase increases.
More specifically, it was found that the evaluation value of the detergency falls relatively slowly from 10 to 8 when the water concentration in the oil phase is in the range of 0 to 5 wt%, while the evaluation value of the detergency starts to fall rapidly when the water concentration in the oil phase exceeds 5 wt%, the evaluation value falls to 5 when the water concentration in the oil phase is 7 wt%, the evaluation value falls to 3 when the water concentration in the oil phase is 10 wt%, and the evaluation value falls to 2 when the water concentration in the oil phase is 15 wt%.
Therefore, it is understood that the water content in the oil phase should be set to a value of 5% by weight or less in order to obtain excellent detergency.
(2) Conductivity in aqueous phase
Further, it is preferable that the electric conductivity (measurement temperature: 25 ℃) in the aqueous phase is set to a value within the range of 0.1 to 300. mu.S/cm.
The reason for this is that if the conductivity is less than 0.1. mu.S/cm, metal ions are readily dissolved therein, and metal influence is likely to occur.
On the other hand, if the conductivity is more than 300. mu.S/cm, the object to be cleaned is likely to be corroded by a potential difference.
Therefore, the lower limit of the electrical conductivity in the aqueous phase is set to a value of more preferably 0.3. mu.S/cm or more, and still more preferably 0.5. mu.S/cm or more.
The upper limit of the electrical conductivity in the aqueous phase is set to a value of 250. mu.S/cm or less, more preferably 200. mu.S/cm or less.
(3) pH in the aqueous phase
Further, it is preferable that the pH (measurement temperature: 25 ℃) in the aqueous phase is set to a value within the range of 4.5 to 9.5.
The reason for this is that if the pH is less than 4.5, the object to be cleaned is likely to be pH-corroded, and the cleaning effect of the flux is significantly reduced.
On the other hand, if the pH is above 9.5, the object to be cleaned may be easily pH-corroded.
Therefore, the lower limit of the pH in the aqueous phase is set to a value of more preferably 5 or more, and still more preferably 5.5 or more.
The upper limit of the pH in the aqueous phase is set to a value of more preferably 9 or less, and still more preferably 8.5 or less.
(4) Flash point and combustion point
Preferably, the cleaning agent composition of the present invention has no flash point, or has a flash point, the temperature of which is set to a value of 40 ℃ or higher and the combustion point of which is set to a value of 60 ℃ or higher.
The reason for this is that if the flash point is 40 ℃ or higher and the combustion point is 60 ℃ or higher, this is not a dangerous article in the fire-fighting law.
However, if the flash point and the flame point of the cleaning agent composition are too high, the kinds and the blending amounts of the 1 st to 4 th organic solvents and the like that can be used may be excessively limited.
Therefore, even when the cleaning agent composition has a flash point, the temperature is set to a value in the range of more preferably 45 to 150 ℃, and more preferably 50 to 100 ℃.
The combustion point of the cleaning agent composition is more preferably in the range of 70 to 200 ℃, and still more preferably in the range of 80 to 150 ℃.
The flash point of the cleaning composition can be measured in accordance with JIS K2265-1 and 4 (method for determining flash point) as described in example 1.
[ 2 nd embodiment ]
1. Preparation step of cleaning agent composition
The preparation step of the detergent composition is a step of preparing the detergent composition described in embodiment 1.
Therefore, the cleaning agent composition may be used as it is when it is prepared, and for example, when only the organic solvent portion (stock solution for cleaning agent composition) is prepared, 50 to 3900 parts by weight of water is mixed with 100 parts by weight of the stock solution for cleaning agent composition to prepare the cleaning agent composition.
2. Cleaning process
(1) Cleaning form
When the cleaning method using the cleaning agent composition is carried out, the cleaning method is not particularly limited, and various methods such as an immersion method, a shaking method, an ultrasonic vibration method, a shower cleaning method, and a submerged jet method can be used.
Further, it is also preferable to clean the flux in a state where the cleaning agent composition is impregnated or adhered to a brush, a cleaning roller, or the like.
In the case of performing a cleaning method using the cleaning agent composition, a cleaning apparatus described later is particularly preferably used.
(2) Cleaning conditions
In addition, in the case of performing a cleaning method using the cleaning agent composition, it is preferable to perform cleaning under conditions of, for example, 30 to 80 ℃ for 10 seconds to 60 minutes.
This is because if a predetermined cleaning effect is obtained under such conditions, thermal deterioration and oxidative deterioration of the cleaning agent composition itself can be effectively prevented.
In order to bring the cleaning agent composition into a cloudy state and to exhibit excellent cleaning performance, it is preferable to bring the cleaning agent composition into a stirred state as one of the cleaning conditions.
More specifically, it is preferable to use a screw stirrer, a magnetic stirrer, or the like, and to stir the detergent composition at a rotation speed in the range of 30 to 1000 rpm.
3. Rinsing procedure
The detergent composition of the present invention has excellent drying properties, and therefore, a rinsing step can be substantially omitted.
However, in cleaning electronic components, substrates, and the like, there are cases where the cleaning agent composition remains and causes galvanic corrosion or the like in the electronic components, substrates, and the like, and therefore it is also preferable to further provide a rinsing step.
In particular, when the cleaning composition contains a hydrophilic amine compound, an alcohol solvent is preferably used as the rinse solution.
The reason for this is that the drying can be performed more quickly than in water, and the influence of metals when the hydrophilic amine compound is mixed can be suppressed.
More specifically, as the alcohol-based solvent, one or two or more kinds of alcohols selected from methanol, ethanol, propanol, isopropanol, butanol, isobutanol, tert-butanol, sec-butanol, aminoalcohol, 1-methoxy-2-propanol, and the like are preferably used.
It is preferable to use an alcohol solvent in which a predetermined amount of water is added to these alcohols, and specifically, an alcohol solvent in which water is added so as to be 40 to 70 wt% based on the whole amount is preferably used.
The rinsing treatment is more preferably carried out in two stages at 5 to 40 ℃ for 1 second to 30 minutes as the rinsing condition. This is because the residue of the surfactant and the amine compound can be further reduced.
However, since there is little problem of deterioration of electrical characteristics of electronic parts, substrates, and the like due to residual surfactant or the like when removing the flux adhering to the solder processing apparatus or the like, the above-mentioned rinsing step can be omitted or simplified.
4. Cleaning device
In the case of performing a cleaning method using the cleaning agent composition, the cleaning apparatus 10 for the flux used preferably includes, for example, a cleaning tank 12, a rinsing tank 14, and a drying tank 16, as shown in fig. 4 (a), and the cleaning tank 12 includes an ultrasonic transducer 29 for ultrasonic cleaning.
More specifically, the cleaning tank 12 is preferably composed of a housing 12a, a storage section 20 for the object 23 to be cleaned, an ultrasonic transducer 29, a cleaning liquid stirring device (not shown), and a heater 19 with a thermostat, and the ultrasonic transducer 29 applies ultrasonic vibration to the cleaning liquid composition 21 that is stirred and circulated, thereby efficiently cleaning the object 23 to be cleaned.
As shown in fig. 4 (b), the cleaning tank 12 is preferably composed of a housing 12a, a storage part 20 for the object 23 to be cleaned, an ultrasonic transducer 29, a cleaning liquid stirring device (not shown), a heater 19 with a thermostat, and a circulation path 22 for circulating a cleaning liquid composition 21.
That is, a part of the contaminated detergent composition 21 may be circulated by the pump 24, and the detergent composition 21 may be regenerated in the filter 28 or the salt-forming compound storage portion 26 provided in the circulation path 22 in the middle thereof.
Next, it is preferable that the rinsing liquid 15 and the like are evaporated and completely removed in the drying tank 16 while the flux and the like are further removed from the object 23 to be cleaned and the cleaning agent composition 21 are removed in the rinsing tank 14.
That is, by using such a cleaning apparatus 10, it is possible to clean electronic components, substrates, and the like subjected to solder treatment using the cleaning agent composition of the present invention, and to efficiently remove flux adhering to them while effectively suppressing metal corrosion.
5. Object to be cleaned
In the case of carrying out the cleaning method using the cleaning agent composition, the kind of the object to be cleaned to which the cleaning agent composition is applied is not particularly limited, and it is needless to say that the electronic component and the substrate subjected to the soldering treatment can be applied, and any component or the like having an influence of the flux can be suitably applied without the soldering treatment.
Thus, specific examples thereof include a printed circuit board, a ceramic wiring board, a semiconductor device (including semiconductor components such as BGA, CSP, PGA, and LGA), a semiconductor device mounting board, a TAB tape with bumps, a TAB tape without bumps, a TAB tape with a semiconductor device mounting, a lead frame, a capacitor, and a resistor.
The object to be cleaned preferably has at least one metal selected from magnesium, aluminum, phosphorus, titanium, chromium, iron, nickel, copper, zinc, germanium, palladium, silver, indium, tin, antimony, platinum, gold, lead, and bismuth, or an alloy containing the metal, on the exposed surface.
The reason for this is that the cleaning method of the present invention can effectively suppress the occurrence of metal corrosion even when the object to be cleaned is the object.
Examples of such objects to be cleaned include a lead frame formed by die bonding a semiconductor element using an aluminum pad, and a mounting board formed by integrating an aluminum heat sink for heat dissipation.
The term "having an exposed surface" is included in the case where the metal or alloy is not exposed to the surface accurately by forming an oxide film or the like.
The type of flux used for these objects to be cleaned is not particularly limited, and for example, a general solder flux may be, of course, preferably a low VOC flux, a flux for lead-free solder, a halogen-free solder flux, a high-melting solder flux, or a no-clean solder flux.
That is, these solder fluxes are usually composed mainly of rosin, and at least one compound selected from organic acid salts, glycidyl ether compounds, oxo acids, carboxylic acids (including dicarboxylic acids), aniline, and thermosetting resins (for example, epoxy resins and thermosetting acrylic resins) is added thereto.
Therefore, if the cleaning method of the present invention is used, it is possible to exhibit excellent cleaning performance not only for a general solder flux but also for these solder fluxes.
The kind of the flux to be added is not particularly limited, and is typically selected from general solders, high-melting-point solders, lead-free solders, and no-clean solders, and examples thereof include Sn-Ag-based solders, Sn-Ag-Cu-based solders, Sn-Sb-based solders, Sn-Zn-based solders, Sn-Bi-based solders, and Pb-Sn-based solders.
[ examples ]
The present invention will be described in detail below with reference to examples. It is to be understood that the present invention is not limited to the following description.
[ example 1]
1. Preparation of stock solution for detergent composition
100 parts by weight of isopropyltoluene (boiling point: 177 ℃ C., solubility in water: 1% by weight or less) as a 1 st organic solvent, 15 parts by weight of 1-hexanol (boiling point: 157 ℃ C., solubility in water: 1% by weight or less) as a 2 nd organic solvent, and 35 parts by weight of N-methyl-2-pyrrolidone (boiling point: 204 ℃ C., solubility in water: 100% by weight or more) as a 3 rd organic solvent were contained in a vessel, and sufficiently stirred to be uniform by using a mixer as a stirring device, thereby preparing a stock solution for a detergent composition of example 1.
Table 1 shows the blending composition of the stock solution for a cleanser composition of example 1.
2. Preparation of detergent composition
The obtained stock solution for a detergent composition and 233.3 parts by weight of water were contained in a vessel and sufficiently stirred by a mixer as a stirring device to prepare a detergent composition.
3. Evaluation of
(1) Evaluation of Water concentration in oil phase
The resulting cleanser composition (200 g) was placed in a 300ml beaker, and then allowed to stand at 25 ℃ for 1 hour.
Next, the water concentration in the oil phase formed by the phase separation was measured using a Karl Fischer moisture meter (MKS-500, manufactured by Kyoto electronics industries Co., Ltd.). The obtained results are shown in table 1.
(2) Evaluation of the conductivity in the aqueous phase
The resulting cleanser composition (200 g) was placed in a 300ml beaker, and then allowed to stand at 25 ℃ for 1 hour.
Then, an aqueous phase was taken out from the oil phase and the aqueous phase formed by the phase separation, and the electric conductivity of the taken-out aqueous phase was measured by using a conductivity meter CEH-12 (manufactured by KOSS corporation). The obtained results are shown in table 1.
(3) Evaluation of pH in aqueous phase
The resulting cleanser composition (200 g) was placed in a 300ml beaker, and then allowed to stand at 25 ℃ for 1 hour.
Next, the aqueous phase was taken out of the oil phase and the aqueous phase formed by the phase separation.
Next, the pH of the taken-out aqueous phase was measured at a measurement temperature of 25 ℃ using a pH meter (M-8, manufactured by horiba, Ltd.). The obtained results are shown in table 1.
(4) Evaluation of Metal Corrosion resistance
The resulting cleansing composition (200 g) was placed in a 300ml beaker, and the temperature was maintained at 50 ℃.
Next, a copper plate 38 was obtained by fixing a semiconductor element 34 having a bonding pad portion (aluminum pad) 32 made of aluminum as a main material shown in (a) to (b) of fig. 5 by solder 36, the copper plate 38 was contained as a test piece 30 in a beaker containing 200g of the cleaning agent composition, and a magnetic stirrer in the beaker was rotated in this state to make the cleaning agent composition in a cloudy state and a corrosion test was performed for a predetermined time.
Subsequently, the rotation of the magnetic stirrer was stopped, and the test piece 30 was taken out of the cleaning agent composition and dried for a predetermined time by using a circulation oven maintained at 100 ℃.
Thereafter, the dried test piece 30 was taken out from the circulating oven, and the surface was visually observed to evaluate the metal corrosion resistance of the cleaning agent composition according to the following criteria. The obtained results are shown in table 1.
Fig. 5 (a) is a plan view of the test piece 30, and fig. 5 (b) is a cross-sectional view of the test piece 30 shown in fig. 5 (a) when viewed in the direction of arrow a, the cross-section being cut by a broken line.
Very good: copper plate and aluminum pad, no change in appearance was observed after 60 minutes of immersion.
O: the copper plate and the aluminum pad showed no change in appearance after 30 minutes of immersion, but showed a change in appearance after 60 minutes of immersion.
And (delta): the copper plate and the aluminum pad, after 15 minutes of immersion, showed no change in appearance, but after 30 minutes of immersion, showed a change in appearance.
X: copper plates and aluminum pads, and the change in appearance was observed after 15 minutes of immersion.
(5) Evaluation of cleaning Property
A commercially available lead-free SOLDER paste ECO SOLDER M705-GRN360-K2-V (available from Kishin Metal industries, Ltd.) was printed and applied onto a JIS2 type comb-shaped substrate through a metal mask.
Next, the comb-shaped substrate on which the solder paste was printed was placed on a hot plate with a lid maintained at 240 ℃, and a commercially available solder paste was reflowed to prepare a test piece.
On the other hand, 200g of the obtained detergent composition was stored in a 300ml beaker and then maintained at 50 ℃.
Next, a plurality of test pieces were housed in a beaker containing a detergent composition, and a cleaning test was performed on the solder paste by rotating a magnetic stirrer in this state to change the cleaning time while the detergent composition was in a cloudy state.
That is, the rotation of the magnetic stirrer was stopped at every predetermined cleaning time, and any one of the test pieces was taken out from the cleaning agent and dried for 10 minutes by using a circulating oven maintained at 100 ℃.
Finally, the dried test piece was taken out from the circulation oven, the surface was observed using a stereomicroscope (magnification 40), the time (cleaning time) for which the solder paste could be completely cleaned was measured, and the cleaning property was evaluated according to the following criteria. The obtained results are shown in table 1.
Very good: the cleaning time is less than 10 minutes.
O: the cleaning time is 10 to less than 15 minutes.
And (delta): the cleaning time is 15-less than 30 minutes.
X: the cleaning time is more than 30 minutes.
(6) Evaluation of drying Property
The resulting cleansing composition (200 g) was placed in a 300ml beaker, and the temperature was maintained at 50 ℃.
Next, the glass epoxy plate was stored in a beaker containing 200g of the detergent composition, and in this state, a magnetic stirrer in the beaker was rotated to conduct a 30-minute cleaning test in a cloudy state of the detergent composition.
Next, the rotation of the magnetic stirrer was stopped, the glass epoxy substrate was taken out from the cleaning agent, and dried for a predetermined time by using a circulation oven maintained at 100 ℃.
Thereafter, the dried glass epoxy substrate was taken out from the circulation oven, and the surface was visually observed to evaluate the drying property of the cleaning agent composition according to the following criteria. The obtained results are shown in table 1.
Very good: drying can be carried out within 5 minutes.
O: drying can be carried out within 10 minutes.
And (delta): some liquid remained under the condition of drying for 10 minutes.
X: a large amount of liquid remained under the condition of drying for 10 minutes.
(7) Flash point
According to JIS K2265-1: 2007 (flash point measurement method (TAG sealing method)) and JIS K2265-4: 2007 (flash point assay (cleveland open cup method)) measures the flash point of the resulting cleaner composition. The obtained results are shown in table 1.
Examples 2 to 12 and comparative examples 1 to 9
Cleaning agent compositions were prepared and evaluated in the same manner as in example 1, except that the compositions of the cleaning agent compositions in examples 2 to 12 and comparative examples 1 to 9 were changed as shown in table 1. The obtained results are shown in table 1.
[ Table 1]
[ Table 1]
TABLE 1
The blending amount (parts by weight) of each component in the stock solution for a cleaning agent composition indicates a value when the 1 st organic solvent is 100 parts by weight.
The numerical values in parentheses in the column of the amounts of the components in the stock solution for the detergent composition indicate the amounts of the components to be mixed (wt%) relative to the total amount of the detergent composition.
The amount of water (parts by weight) in the detergent composition indicates the amount of water added per 100 parts by weight of the stock solution for detergent composition.
The number in parentheses in the column of the amount of water blended in the detergent composition indicates the amount of water blended (wt%) relative to the total amount of the detergent composition.
The 4 th organic solvent contains N-ethylethanolamine among the organic solvents described in the section "other organic solvents
Industrial applicability
According to the detergent composition of the present invention, the predetermined hydrophobic organic solvent as the 1 st organic solvent and the 2 nd organic solvent, the predetermined hydrophilic organic solvent as the 3 rd organic solvent, and water are blended at a predetermined ratio, and the hydrophilic amine compound as the 4 th organic solvent is not contained or is contained in a range smaller than a predetermined range in some cases, and is in a substantially amine-less (amine) state, and the water concentration in the oil phase at the time of phase separation is made to be a predetermined range or less, whereby the detergent composition is excellent in environmental safety, can exhibit excellent detergency, and can effectively suppress metal corrosion of the object to be cleaned.
Therefore, according to the cleaning agent composition of the present invention and the cleaning method using the cleaning agent, even when cleaning of electronic parts and the like, in particular, lead frames obtained by soldering semiconductor elements using aluminum pads, in which metal corrosion is likely to occur and is fatal, is performed, flux residue can be removed with high accuracy and stability in consideration of environmental problems.
Description of the symbols
10: cleaning device
12: cleaning tank
14: flushing tank
15: washing liquid
16: drying trough
21: cleaning liquid
22: circulation path
26: salt-forming compound reservoir
28: filter
29: ultrasonic vibrator
30: test piece for evaluating metal corrosion resistance
31: polyimide protective film
32: aluminum pad
34: semiconductor component
36: soldering tin
38: copper plate
Claims (6)
1. A detergent composition for cleaning an object to be cleaned in a cloudy state,
containing 1 st to 4 th organic solvents and water, and
the 1 st organic solvent is at least one compound selected from the group consisting of hydrophobic aromatic compounds, hydrophobic terpene compounds and hydrophobic cycloalkane compounds, the solubility of which in water is 10 wt% or less, wherein the solubility measurement temperature is 20 ℃, and the compound is selected from the group consisting of indene, hemimellitene, pseudocumene, mesitylene, cumene, methylisoprene, phenetole, limonene, alpha-pinene and p-pinene
Alkane, decahydronaphthalene, octahydroindenePinane, p
More than 1 of the mixture of diene isomer mixture and C9 alkylcyclohexane,
the 2 nd organic solvent is a hydrophobic monohydric alcohol compound having a solubility in water of 10 wt% or less, wherein the solubility is measured at 20 ℃ and is at least 1 selected from the group consisting of 1-hexanol, methyl pentanol, 2-ethyl butanol, methyl isobutyl carbinol, cyclohexanol, 1-heptanol, 2-heptanol, 3-heptanol, 4-heptanol, 2-methyl cyclohexanol, benzyl alcohol, 1-octanol, 2-ethylhexanol, 2-nonanol, diisobutyl carbinol, and 3,5, 5-trimethylhexanol,
the 3 rd organic solvent is a hydrophilic nitrogen-containing compound and a hydrophilic sulfur-containing compound having a solubility in water of 50 wt% or more, or any one of them, wherein the solubility is measured at 20 ℃ at 1 or more selected from the group consisting of N-methyl-2-pyrrolidone, N-ethyl-2-pyrrolidone, dimethyl sulfoxide, dimethylacetamide, N-dimethylformamide, and N, N-diethylformamide,
the 4 th organic solvent is a hydrophilic amine compound having a solubility in water of 50 wt% or more, wherein the solubility is measured at 20 ℃ and is 1 or more selected from the group consisting of N, N-diethylisopropanolamine, N-methylethanolamine, monoisopropanolamine, N-diethylethanolamine, N-ethylethanolamine, and N-t-butylethanolamine,
the amount of the 2 nd organic solvent is set to a value within a range of 3 to 100 parts by weight based on 100 parts by weight of the 1 st organic solvent,
the amount of the 3 rd organic solvent is set to a value within the range of 3 to 100 parts by weight based on 100 parts by weight of the 1 st organic solvent,
the 4 th organic solvent is added in an amount of less than 0.1 part by weight based on 100 parts by weight of the 1 st organic solvent,
the amount of water is 50 to 3900 parts by weight based on 100 parts by weight of the total amount of organic solvents,
and when the phase separation is carried out between an oil phase and an aqueous phase, the water concentration in the oil phase is set to a value of 5% by weight or less, wherein the measurement temperature of the water concentration is 25 ℃.
2. The cleaning agent composition according to claim 1, wherein the electrical conductivity in the aqueous phase is adjusted to a value in the range of 0.1 to 300. mu.S/cm, and wherein the measurement temperature of the electrical conductivity is 25 ℃.
3. The cleaning agent composition according to claim 1, wherein the pH in the aqueous phase is adjusted to a value in the range of 4.5 to 9.5, and wherein the measurement temperature of the pH is 25 ℃.
4. The cleaning agent composition according to claim 1, wherein the boiling point of the 1 st organic solvent is set to a value in the range of 140 to 210 ℃, the boiling point of the 2 nd organic solvent is set to a value in the range of 130 to 220 ℃, and the boiling point of the 3 rd organic solvent is set to a value in the range of 150 to 220 ℃.
5. The cleaning agent composition according to claim 1, wherein the object to be cleaned has at least one metal selected from the group consisting of magnesium, aluminum, phosphorus, titanium, chromium, iron, nickel, copper, zinc, germanium, palladium, silver, indium, tin, antimony, platinum, gold, lead and bismuth, or an alloy containing the metal, on the exposed surface.
6. A cleaning method comprising cleaning an object to be cleaned by bringing the cleaning agent composition according to any one of claims 1 to 5 into a cloudy state.
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| US12005646B2 (en) * | 2019-05-22 | 2024-06-11 | Raiser Moon, Inc. | Cleaning method, cleaning device, cleaning agent, and preliminary cleaning agent |
| US11584900B2 (en) | 2020-05-14 | 2023-02-21 | Corrosion Innovations, Llc | Method for removing one or more of: coating, corrosion, salt from a surface |
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| CN101955858A (en) * | 2009-07-17 | 2011-01-26 | 日东电工株式会社 | Die cleaning agent composition and mould cleaning material and the mould cleaning method that uses it |
| CN102906240B (en) * | 2010-07-09 | 2014-12-10 | 化研科技株式会社 | Liquid concentrate for cleaning composition, cleaning composition and cleaning method |
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| JP2639733B2 (en) | 1989-07-31 | 1997-08-13 | 花王株式会社 | Detergent composition |
| US5393451A (en) * | 1991-01-11 | 1995-02-28 | Koetzle; A. Richard | High temperature flashpoint, stable cleaning composition |
| JP5565939B2 (en) * | 2009-01-26 | 2014-08-06 | 化研テック株式会社 | Stock solution for cleaning composition, cleaning composition, and cleaning method |
| JP5546263B2 (en) * | 2009-01-26 | 2014-07-09 | 化研テック株式会社 | Cleaning liquid regenerating device and circulating cleaning device |
| JP6226144B2 (en) * | 2014-02-27 | 2017-11-08 | 荒川化学工業株式会社 | Detergent composition stock solution, detergent composition and cleaning method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101955858A (en) * | 2009-07-17 | 2011-01-26 | 日东电工株式会社 | Die cleaning agent composition and mould cleaning material and the mould cleaning method that uses it |
| CN102906240B (en) * | 2010-07-09 | 2014-12-10 | 化研科技株式会社 | Liquid concentrate for cleaning composition, cleaning composition and cleaning method |
| CN104312779A (en) * | 2010-07-09 | 2015-01-28 | 化研科技株式会社 | Liquid concentrate for cleaning composition, cleaning composition and cleaning method |
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| US20190048294A1 (en) | 2019-02-14 |
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